Emetine salts and process of making same.



NITED STATES PATENT FFIcEi \VILLIAM GEORGE WHIFFEN, OF LONDON, ENGLAND.

EMETINE SALTS AND PROCESS OF MAKING SAME.

SPECIFICATION forming part of Letters Patent No. 650,696, dated May 29,1900.

Application filed June 2, 1898. Serial No. 682,418. (No specimens.)

T0 aZZ whmn it may concern:

Be it known that I, WILLIAM GEORGE WVHIFFEN, manufacturing chemist, asubject of the Queen of Great Britain, residing at Battersea, in thecity of London, England, have invented a new and useful Process for thePreparation of Emetine, (for which I applied for Letters Patent in GreatBritain on the 12th of November, 1897, No. 26,442, and in Germany on thel6th'of November, 1897,) of which the following is a specification.

My invention relates to an improved process for obtaining the alkaloidof ipecacuanha, known as emetine. This alkaloid has hitherto beenobtainable in the pure state, or ap proximatelypure state, only by greatcare and trouble and at very considerable cost in the form of thehydrochlorate, and the commercial salt thus obtained is usually more orless impure and contaminated with excess of acid. By myinvention Ireadily produce a perfectlyneutral crystalline salt of emetine of greatpurity and entirely free from cephaeline, and therefore well suited forvarious purposes to which the present hydrochlorate salt isinapplicable.

I have discovered by experiment and research that the hydrobromate ofe'metine is a salt possessing special qualities, and particularly thatit crystallizes readily, whereas the hydrobromate of cephaelinecrystallizes with difficulty and the hydrobromates of certain otheralkaloids, more or less present in the root, are uncrystallizable.

In carrying myinvention into effect I prefer to operate as follows: Thefinely-powdered root is mixed intimately with about ten per cent. oflime and the whole is moistened with Water. The mixture is thenextracted by warm amylic alcohol or by ether or by a suitablehydrocarbon immiscible with water. The immiscible solution is thenagitated with a weak aqueous solution of hydrobromic acid and theaqueous solution concentrated suffr ciently for the emetine hydrobromateto crystallize upon cooling. These crystals are almost pure and themother-liquor contains the other alkaloids present. The hydrobromate ofemetine is finally treated with animal charcoal and further purified byrecrystallization from Water, whereby a neutral salt is produced in astate of purity unobtainable by any other known means.

The reaction between the extract of the root and the hydrobromic-acidsolution may be aided, if needful, by means of heat, or, if

found desirable, in certain cases I may effect the reaction in the coldand condense the resulting liquid by other means than by heating-as, forinstance, by evaporation in 'uacuo at or about the ordinary atmospherictemperature.

What I claim is- 1. The process for treating fluid extract ofipecacuanha-root, which consists in adding aqueous solution ofhydrobromic acid to the said extract, agitating the liquids together,concentrating the aqueous solution until hydrobromate of emetinecrystallizes out, and separating the crystals from the motherliquor.

v 2. The process for separating emetine from other alkaloids ofipecacuanha-root,'which consists in treating the root with lime,extracting the alkaloids by a solvent immiscible with water, treatingthe solution with aqueous solution of hydrobromic acid, andconcentrating the said aqueous solution to separation of the emetine asa crystalline compound, the cephaeline remaining in solution.

3. As a new chemical product crystals of hydrobromate of emetine andwater of crystallization.

In witness whereof I have hereunto set my hand in presence of twowitnesses.

WILLIAM GEORGE WHIFFEN.

Witnesses:

GEORGE HUGHES, W. M. HARRIS.

